CN107302054B - Double heterojunction optical detector and preparation method thereof - Google Patents
Double heterojunction optical detector and preparation method thereof Download PDFInfo
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- CN107302054B CN107302054B CN201710411589.8A CN201710411589A CN107302054B CN 107302054 B CN107302054 B CN 107302054B CN 201710411589 A CN201710411589 A CN 201710411589A CN 107302054 B CN107302054 B CN 107302054B
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Abstract
The present invention relates to a kind of preparation methods of double heterojunction optical detector, comprising: (a) cleans semi-insulating translucent substrate；(b) bottom electrode layer is grown over the substrate；(c) one MoS of growth regulation on the bottom electrode layer2Layer；(d) in the first MoS2Hydridization calcium titanium ore bed is grown on layer；(e) two MoS of growth regulation on the hydridization calcium titanium ore bed2Layer；(f) in the 2nd MoS2Top electrode is grown on layer.Hydridization perovskite double heterojunction of the present invention can make the completely depleted of the background carriers of two-dimensional material channel, significantly reduce device dark current, improve detection performance of the device under dim light；Preparation process is simple, and production cost is low, the advantages that without expensive instrument and equipment；The photodetector of preparation can work under zero grid voltage, low source and drain bias, have excellent low power consumption characteristic, and structure is simple, high-efficient, response is fast, the operation is stable, long service life.
Description
Technical field
The invention belongs to semiconductor optoelectronic detection technology fields, and in particular to a kind of double heterojunction optical detector and its preparation
Method.
Background technique
Using graphene and two-dimentional Transition-metal dichalcogenide as the two-dimensional material of representative in photodetection field by more
Carry out more extensive concern.Wherein with molybdenum disulfide (MoS2) be representative transient metal sulfide two-dimensional material have and silicon, arsenic
Change the close forbidden bandwidths of conventional semiconductor materials such as gallium, and energy band band gap changes with the variation of thickness, is visited in novel photoelectric
Survey field has broad prospect of application.However this kind of material inevitably introduces the problems such as boundary defect during the preparation process
So that material concentration of background carriers with higher under zero grid voltage, so that the dark current of photodetector is higher,
These problems all limit it in the application in photodetection field.
Therefore, it is particularly important that a kind of low-dark current, the optical detector of high detection performance how to be developed.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the present invention provides a kind of double heterojunction optical detector and its
Preparation method.
An embodiment provides a kind of double heterojunction optical detectors, comprising:
A kind of preparation method of double heterojunction optical detector characterized by comprising
(a) semi-insulating translucent substrate is cleaned；
(b) bottom electrode layer is grown over the substrate；
(c) one MoS of growth regulation on the bottom electrode layer2Layer；
(d) in the first MoS2Hydridization calcium titanium ore bed is grown on layer；
(e) two MoS of growth regulation on the hydridization calcium titanium ore bed2Layer；
(f) in the 2nd MoS2Top electrode is grown on layer.
In one embodiment of the invention, step (a) includes:
(a1) semi-insulating translucent single-sided polishing material is chosen as the substrate；
(a2) substrate is cleaned using RCA standard cleaning technique.
In one embodiment of the invention, the substrate material is sapphire.
In one embodiment of the invention, step (b) includes:
(b1) magnetron sputtering technique is utilized, sputters first metal material in the burnishing surface of the substrate；
(b2) under the atmosphere of nitrogen and argon gas, using rapid thermal anneal process, make the burnishing surface of the substrate with it is described
Ohmic contact is formed at first metal material surface to complete the growth of the bottom electrode layer.
In one embodiment of the invention, step (d) includes:
(d1) precursor solution is prepared；
(d2) precursor solution is stirred and is spin-coated to the first MoS2To grow hydridization calcium titanium ore bed on layer.
In one embodiment of the invention, the material of the hydridization calcium titanium ore bed is CH3NH3PbI3。
In one embodiment of the invention, step (e) uses lower temperature growth process, and the lower temperature growth process temperature is small
In 150 degree.
In one embodiment of the invention, the first MoS2Layer and the 2nd MoS2The growth technique of layer is magnetic
Control sputtering technology.
In one embodiment of the invention, step (f) includes:
(f1) physical mask plate is used, using magnetron sputtering technique in the 2nd MoS2Two metal material of growth regulation on layer
Material；
(f2) under the atmosphere of nitrogen and argon gas, using rapid thermal anneal process, in the 2nd MoS2The upper surface of layer
The growth of the top electrode is completed with formation Ohmic contact at second metal material surface.
A kind of double heterojunction optical detector is proposed in another embodiment of the invention, comprising: semi-insulating translucent lining
Bottom, bottom electrode layer, the first MoS2Layer, hydridization calcium titanium ore bed, the 2nd MoS2Layer, top electrode, the double heterojunction optical detector by
Method described in above-described embodiment prepares to be formed.
Compared with prior art, the invention has the following advantages:
1, hydridization perovskite double heterojunction can make the completely depleted of the background carriers of two-dimensional material channel, significantly reduce
Device dark current improves detection performance of the device under the dim light；
2, preparation process is simple, and production cost is low, the advantages that without expensive instrument and equipment；
3, the photodetector prepared can work under zero grid voltage, low source and drain bias, have excellent low power consumption characteristic, and
Structure is simple, high-efficient, response is fast, the operation is stable, long service life.
Detailed description of the invention
Fig. 1 is a kind of preparation method flow chart of double heterojunction optical detector provided in an embodiment of the present invention；
Fig. 2 a~Fig. 2 f is a kind of process flow diagram of double heterojunction optical detector provided in an embodiment of the present invention；
Fig. 3 is a kind of structural schematic diagram of double heterojunction optical detector provided in an embodiment of the present invention；
Fig. 4 is a kind of MoS provided in an embodiment of the present invention2Raman scattering figure；
Fig. 5 is a kind of luminescence generated by light figure of hydridization perovskite provided in an embodiment of the present invention.
Specific embodiment
Further detailed description is done to the present invention combined with specific embodiments below, but embodiments of the present invention are not limited to
This.
Embodiment one
Referring to Figure 1, Fig. 4 and Fig. 5, Fig. 1 are a kind of preparation of double heterojunction optical detector provided in an embodiment of the present invention
Method flow diagram；Fig. 4 is a kind of MoS provided in an embodiment of the present invention2Raman scattering figure；Fig. 5 provides for the embodiment of the present invention
A kind of hydridization perovskite luminescence generated by light figure.
This method comprises the following steps:
(a) semi-insulating translucent substrate is cleaned；
(b) bottom electrode layer is grown over the substrate；
(c) one MoS of growth regulation on the bottom electrode layer2Layer；
(d) in the first MoS2Hydridization calcium titanium ore bed is grown on layer；
(e) two MoS of growth regulation on the hydridization calcium titanium ore bed2Layer；
(f) in the 2nd MoS2Top electrode is grown on layer.
Wherein, step (a) includes:
(a1) semi-insulating translucent single-sided polishing material is chosen as the substrate；
(a2) substrate is cleaned using RCA standard cleaning technique.
Preferably, the substrate material is sapphire.
Wherein, step (b) includes:
(b1) magnetron sputtering technique is utilized, sputters the first metal material in the burnishing surface of the substrate；
(b2) under the atmosphere of nitrogen and argon gas, using rapid thermal anneal process, make the burnishing surface of the substrate with it is described
Ohmic contact is formed at first metal material surface to complete the growth of the bottom electrode layer.
Wherein, the material of the bottom electrode layer and the top electrode can be gold, silver, nickel, titanium, platinum, palladium, FTO, ITO electricity
One of pole is a variety of, and as extraction electrode, is connected with external circuit.
Preferably, the bottom electrode layer is ITO electrode.
Wherein, step (d) includes:
(d1) liquid solution is driven in preparation；
(d2) the drive liquid solution is stirred and is spin-coated to the first MoS2To grow hydridization calcium titanium ore bed on layer.
Wherein, the hydridization calcium titanium ore bed material is organic or inorganic hybridization perovskite, including CH3NH3PbI3、
CH3NH3PbCl3、CH3NH3SnI3Etc., it is weak p-type, carrier concentration 1016cm-3Magnitude；Growing method is a step solution
One of method, two step solwution methods, coevaporation method.
Preferably, the material of the hydridization calcium titanium ore bed is CH3NH3PbI3。
Wherein, the hydridization calcium titanium ore bed with a thickness of 200-350nm.
Wherein, step (e) uses lower temperature growth process, and the lower temperature growth process temperature is less than 150 degree.
Wherein, the first MoS2Layer and the 2nd MoS2Layer is single layer or multilayered film material, carrier type choosing
Use N-shaped；Growing method is one of magnetron sputtering, chemical vapor deposition, molecular beam epitaxy or spin coating.
Preferably, the first MoS2Layer and the 2nd MoS2The growth technique of layer is magnetron sputtering technique.
Wherein, the first MoS2Layer with a thickness of 1-10nm, the 2nd MoS2Layer with a thickness of 0.5-1nm.
Wherein, step (f) includes:
(f1) physical mask plate is used, using magnetron sputtering technique in the 2nd MoS2Second metal is grown on layer
Material；
(f2) under the atmosphere of nitrogen and argon gas, using rapid thermal anneal process, in the 2nd MoS2The upper surface of layer
The growth of the top electrode is completed with formation Ohmic contact at second metal material surface.
Wherein, the thickness of the bottom electrode layer and the top electrode is 50-200nm.
The present embodiment has the beneficial effect that:
1, double heterojunction can make the completely depleted of the background carriers of two-dimensional material channel, significantly reduce device dark electricity
Stream improves detection performance of the device under dim light；
2, preparation process is simple, and production cost is low, the advantages that without expensive instrument and equipment；
3, the photodetector prepared can work under zero grid voltage, low source and drain bias, have excellent low power consumption characteristic, and
Structure is simple, high-efficient, response is fast, the operation is stable, long service life.
Embodiment two
Referring to Fig. 2 a~Fig. 2 f, Fig. 2 a~Fig. 2 f is a kind of double heterojunction optical detector provided in an embodiment of the present invention
Process flow diagram.This method comprises the following steps:
Step 1 chooses Sapphire Substrate 201, as shown in Figure 2 a.
Step 2 forms bottom electrode layer 202 in 201 first metal material of surface deposition of Sapphire Substrate, such as Fig. 2 b institute
Show.
Step 3 forms the first MoS on 202 surface of bottom electrode layer2Layer 203 i.e. light absorbing layer 1, as shown in Figure 2 c.
Step 4, in the first MoS2It is light absorbing layer 2 that 203 surface of layer, which form hydridization calcium titanium ore bed 204, such as Fig. 2 d institute
Show.
Step 5 forms the 2nd MoS on 204 surface of hydridization calcium titanium ore bed2Layer 205 i.e. light absorbing layer 3, such as Fig. 2 e institute
Show.
Step 6, in the 2nd MoS2205 upper surface of layer deposit the second metal material and form top electrode 206 and dispatch from foreign news agency
Road, as shown in figure 2f.
Wherein, step 1 may include:
Step 1-1, semi-insulating translucent single-sided polishing material is chosen as the Sapphire Substrate 201；
Step 1-2, the Sapphire Substrate 201 is cleaned using RCA standard cleaning technique.
Step 2 may include:
Step 2-1, the first metal is sputtered using the burnishing surface of magnetron sputtering technique Sapphire Substrate 201 described in step 1
Material；
Step 2-2, under the atmosphere of nitrogen and argon gas, using rapid thermal anneal process in the Sapphire Substrate 201
Ohmic contact is formed at burnishing surface and first metal material surface to complete the preparation of the bottom electrode layer 202.
Further, step 2-1 may include: that sputtering is passed through using argon gas as sputter gas using Ti material as target
It is 80W in operating power, vacuum degree is 5 vacuum degrees in cavity-4~64 reciprocal of duty cycles-3Under conditions of Pa, in the Sapphire Substrate
201 burnishing surface sputters the Ti material using as first metal material.
Step 3 may include:
Step 3-1, by the first MoS2Layer 203 i.e. MoS2Film is transferred on bottom electrode layer 202 described in step 2；
Wherein, transfer method are as follows: be grown on original preparation MoS2The first MoS on the substrate of film2203 surface of layer are logical
Cross spin coating or spray on polymer solution production supporting layer, or by by the direct hot pressing of macromolecule membrane in the first MoS2Layer
Be supported layer on 203, then by supporting layer together with the first MoS2Layer 203 is together from its original preparation MoS2It is shelled on the substrate of film
From getting off, it is transferred on bottom electrode layer 202, makes the first MoS2Layer 203 is contacted with bottom electrode layer 202, removes supporting layer.
Step 4 may include:
Step 4-1, by the CH of 0.415g3NH3The PbI of I and 1.223g2It is dissolved in preparation spin coating forerunner in the DMF solution of 4mL
Liquid solution stirs 10-12h in 50；
Step 4-2, precursor solution described in step 4-1 is spun to first described in step 3 with the revolving speed of 3000rpm
MoS2On layer 203；
Step 4-3, anneal 0.5h under 903, and CH is made3NH3PbI3Film, as hydridization calcium titanium ore bed 204.
Step 5 may include:
Step 5-1, due to 204 non-refractory of hydridization calcium titanium ore bed, in two MoS of growth regulation2Low temperature is used when layer 205
Technique growth technique, wherein temperature needs to be less than 150 degree, can be grown using magnetron sputtering technique in hydridization calcium titanium ore bed 204
MoS2Material forms the 2nd MoS2Layer 205.
Further, step 5-1 may include: by MoS2Target is placed on the target position of rf magnetron sputtering system, will
Cavity is evacuated to vacuum state (5 × 10-6Pa), heats entire sample, is passed through gas Ar, adjusts the pressure in vacuum chamber；Wherein,
MoS2Target is 10 centimetres, sputtering power 60-80W, sedimentation time 0.5-1h at a distance from Sapphire Substrate 201.
Step 6 may include:
Step 6-1, using physical mask plate, using magnetron sputtering technique in the 2nd MoS2Described second is grown on layer 205
Metal material；
Step 6-2, under the atmosphere of nitrogen and argon gas, using rapid thermal anneal process in the 2nd MoS2The upper table of layer 205
Ohmic contact is formed at face and second metal material surface to complete the preparation of the top electrode 206.
Step 6-3, the connection of external circuit is completed；
Wherein, step 6-1 may include: to be passed through sputter chamber using argon gas as sputter gas using Au material as target
In, it is 60~80W in operating power, is 5 × 10 in vacuum degree-4~6 × 10-3Under conditions of, in the 2nd MoS2205 table of layer
Face sputters to form the Au top electrode 206.
The present embodiment has the following beneficial effects:
1、MoS2The advantages of be MoS2It is direct band-gap semicondictor, photon directly can be transformed into electron-hole pair,
MoS2The speed of service of the electronics in plane lamina, MoS2Electron transfer rate be about 100cm2/ vs, this is significantly larger than
The mobility of organic inorganic hybridization perovskite can greatly increase photoconduction, while MoS2Material forbidden bandwidth is adjustable, to close red
Outer light is more sensitive.
2, for organic inorganic hybridization perovskite material because its carrier diffusion length is long, the absorption coefficient of light is big, forbidden bandwidth can
It adjusts and is very suitable to Visible-to-Near InfaRed optical detection, dark current is small, small noise current is as the preferred of photodetector material.
3, using double-heterostructure can effectively reduce leakage current to form double potential barrier, to greatly improve photoelectricity
The device reliability of detector, while the separation of photo-generate electron-hole can be promoted.
4, structure is simple, high-efficient, response is fast, the operation is stable, long service life；The preparation process of optical detector is simple,
Production cost is low, the advantages that without expensive instrument and equipment.
Embodiment three
It is a kind of double heterojunction optical detection provided in an embodiment of the present invention referring again to Fig. 2 a~Fig. 2 f, Fig. 2 a~Fig. 2 f
The process flow diagram of device.This method comprises the following steps:
S01: substrate 201 cleans: semi-insulating translucent Sapphire Substrate 201 is placed in acetone, ethyl alcohol and deionized water
It is cleaned by ultrasonic respectively, and is dried in vacuo, as shown in Figure 2 a.
S02: target and substrate 201 are placed: Sapphire Substrate 201 cleaned in step S01 is fixed on sample
On pallet, vacuum chamber is put into, ITO target is placed on to the target position of rf magnetron sputtering system, start to vacuumize.
S03: deposit ITO bottom electrode layer 202: cavity is first evacuated to vacuum state, and (i.e. pressure is 5 × 10-6Pa), heating is blue
Jewel substrate 201 adjusts intracavitary air pressure: where ITO target is 10 centimetres at a distance from Sapphire Substrate 201, and sputtering power is
50W, sedimentation time 0.5h-1h, to complete the preparation of ITO bottom electrode layer 202, as shown in Figure 2 b.
S04: the one MoS2Layer 203 deposits: chemical vapour deposition technique is used, with the molybdenum of simple substance and sulphur powder as source,
Two dimension MoS is deposited on 202 surface of bottom electrode layer2, wherein depositing temperature are as follows: and 800 DEG C -850 DEG C, sedimentation time 0.5-1h, with
Complete the first MoS2The deposit of layer 203, as shown in Figure 2 c.
S05: spin coating hydridization calcium titanium ore bed 204: the DMF that the PbI2 of the CH3NH3I of 0.415g and 1.223g is dissolved in 4mL is molten
Spin coating precursor solution is prepared in liquid, and stirs 10-12h in 50, and precursor solution is spun to by step with the revolving speed of 3000rpm
First MoS described in rapid S042On layer 203, then in the 90 right lower 0.5h that anneal, CH is made3NH3PbI3Film, to complete hydridization
The preparation of calcium titanium ore bed 204, as shown in Figure 2 d.
S06: the two MoS2Layer 205 deposits: by MoS2Target is placed on the target position of rf magnetron sputtering system, by cavity
Being evacuated to vacuum state, (i.e. pressure is 5 × 10-6Pa), heating includes substrate 201, bottom electrode layer 202, the first MoS2Layer 203, hydridization
The entire substrate of calcium titanium ore bed 204, heating temperature are passed through inert gas less than 150 degrees Celsius, adjust the pressure in vacuum chamber；
Wherein, MoS2Target is 10 centimetres, sputtering power 60-80W, sedimentation time 0.5-1h, with complete at a distance from entire substrate
At the 2nd MoS2The deposit of layer 205, as shown in Figure 2 e.
S07: deposit top electrode 206: using mask plate and by radiofrequency magnetron sputtering technology in the 2nd MoS2Above layer 205
Deposit a layer thickness be 100nm Au membrane electrode as test electrode, first by cavity be evacuated to vacuum state (i.e. pressure be 5 ×
10-6Pa), sample is heated, intracavitary air pressure is adjusted: where target is 10 centimetres, sputtering power 50W at a distance from sample, deposition
Time is 1h-2h, to complete the preparation of top electrode 206, as shown in figure 2f.
Example IV
Fig. 3 is referred to, Fig. 3 is a kind of structural schematic diagram of double heterojunction optical detector provided in an embodiment of the present invention；It should
Double heterojunction optical detector successively includes: semi-insulating translucent substrate layer 301, bottom electrode layer 302, the first MoS2Layer 303, hydridization
Calcium titanium ore bed 304, the 2nd MoS2Layer 305, top electrode 306, wherein the double heterojunction optical detector is as described in above-described embodiment
Method prepare to be formed.
Wherein, semi-insulating translucent substrate 301 is single throwing Sapphire Substrate；First MoS2Layer 303 and the 2nd MoS2Layer
305 be single-layer or multi-layer thin-film material, and carrier type selects N-shaped；The hydridization calcium titanium ore bed 304 is CH3NH3PbI3、
CH3NH3PbCl3、CH3NH3SnI3Equal materials are weak p-type, carrier concentration 1016cm-3Magnitude.
Further, the bottom electrode layer 302 and top electrode 306 be Au, Al, Ti, Sn, Ge, In, Ni, Co, Pt, W, Mo,
The metal materials such as Cr, Cu, Pb are formed comprising the conductive compounds such as two or more alloy or bottom in these metals.In addition, can also
To be with 2 layers of structure being made of two or more different metals, such as Al/Ti.The bottom electrode layer 302 be Au, Al, Ti,
The metal materials such as Sn, Ge, In, Ni, Co, Pt, W, Mo, Cr, Cu, Pb include the conductions such as two or more alloy or bottom in these metals
Property compound is formed.Alternatively, it is also possible to being folded with 2 layers of structure being made of different 2 kinds and the above metal, such as Al/Ti
Layer bimetallic material.
In conclusion specific case used herein is to a kind of double heterojunction optical detector of the present invention and preparation method thereof
Principle and embodiment be expounded, method and its core of the invention that the above embodiments are only used to help understand
Thought is thought；At the same time, for those skilled in the art in specific embodiment and applies model according to the thought of the present invention
Place that there will be changes, in conclusion the contents of this specification are not to be construed as limiting the invention, protection of the invention
Range should be subject to the attached claims.
Claims (10)
1. a kind of preparation method of double heterojunction optical detector characterized by comprising
(a) semi-insulating translucent substrate is cleaned；
(b) bottom electrode layer is grown over the substrate；
(c) one MoS of growth regulation on the bottom electrode layer2Layer；
(d) in the first MoS2Hydridization calcium titanium ore bed is grown on layer, wherein the hydridization calcium titanium ore bed is weak p-type, carrier
Concentration is 1016cm-3Magnitude；
(e) two MoS of growth regulation on the hydridization calcium titanium ore bed2Layer；
(f) in the 2nd MoS2Top electrode is grown on layer.
2. preparation method according to claim 1, which is characterized in that step (a) includes:
(a1) semi-insulating translucent single-sided polishing material is chosen as the substrate；
(a2) substrate is cleaned using RCA standard cleaning technique.
3. preparation method according to claim 1, which is characterized in that the substrate material is sapphire.
4. preparation method according to claim 1, which is characterized in that step (b) includes:
(b1) magnetron sputtering technique is utilized, sputters the first metal material in the burnishing surface of the substrate；
(b2) under the atmosphere of nitrogen and argon gas, using rapid thermal anneal process, make the burnishing surface and described first of the substrate
Ohmic contact is formed at metal material surface to complete the growth of the bottom electrode layer.
5. preparation method according to claim 1, which is characterized in that step (d) includes:
(d1) precursor solution is prepared；
(d2) precursor solution is stirred and is spin-coated to the first MoS2To grow hydridization calcium titanium ore bed on layer.
6. preparation method according to claim 1, which is characterized in that the material of the hydridization calcium titanium ore bed is
CH3NH3PbI3。
7. preparation method according to claim 1, which is characterized in that step (e) uses lower temperature growth process, the low temperature
The temperature of growth technique is less than 150 degree.
8. preparation method according to claim 1, which is characterized in that the first MoS2Layer and the 2nd MoS2Layer
Growth technique is magnetron sputtering technique.
9. preparation method according to claim 1, which is characterized in that step (f) includes:
(f1) physical mask plate is used, using magnetron sputtering technique in the 2nd MoS2Two metal material of growth regulation on layer；
(f2) under the atmosphere of nitrogen and argon gas, using rapid thermal anneal process, in the 2nd MoS2Layer upper surface with it is described
Ohmic contact is formed at second metal material surface to complete the growth of the top electrode.
10. a kind of double heterojunction optical detector characterized by comprising semi-insulating translucent substrate layer, bottom electrode layer, first
MoS2Layer, hydridization calcium titanium ore bed, the 2nd MoS2Layer, top electrode, wherein the optical detector is by any one of claim 1~9 institute
The method stated prepares to be formed.
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| CN108365099A (en) * | 2018-01-15 | 2018-08-03 | 复旦大学 | A kind of high performance calcium titanium ore/organic semiconductor heterojunction type photodetector |
| CN108574050B (en) * | 2018-07-04 | 2022-02-15 | 河南师范大学 | Perovskite-MoS2Preparation method of bulk heterojunction perovskite solar cell |
| CN109638091B (en) * | 2018-11-17 | 2020-07-10 | 华中科技大学 | Construction method and regulation and control strategy of high-performance hybrid photoelectric detector |
| CN111477716B (en) * | 2020-04-14 | 2021-07-27 | 合肥工业大学 | 1T-phase tungsten sulfide bipolar heterojunction narrow-band near-infrared photoelectric detector and preparation method thereof |
| CN111640768B (en) * | 2020-05-09 | 2021-06-25 | 北京科技大学 | Vertical double-heterojunction optical detector area array and manufacturing method thereof |
| CN112349840A (en) * | 2020-09-16 | 2021-02-09 | 西安电子科技大学 | Perovskite photoelectric detector and preparation method thereof |
| CN112909126B (en) * | 2021-02-02 | 2022-10-25 | 中南大学 | PVK-TMDCs van der Waals heterojunction and preparation method thereof |
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